CN114678201A - Preparation method of novel high-weather-resistance resin-coated magnetic metal powder - Google Patents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/026—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
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Abstract
The invention relates to the field of metal pigments for wave-absorbing coatings, in particular to a preparation method of novel high-weather-resistance resin-coated magnetic metal powder. The invention coats the magnetic metal powder by selecting the resin which is a material not used for modifying the magnetic metal powder in the industry, and the weather resistance of the coated magnetic metal powder is enhanced without causing obvious deterioration of the imaginary part of the magnetic conductivity and the imaginary part of the dielectric constant by designing the process conditions. The method has the advantages of simple and mature process, strong operability and lower cost, and is suitable for large-scale production. The coated magnetic metal powder has uniform and compact surface, and compared with the similar coated magnetic metal powder, the electromagnetic parameter change of the coated magnetic metal powder is small, the weather resistance is obviously enhanced, and the salt spray resistance time of the wave-absorbing coating prepared by the coated magnetic metal powder can reach more than 3000 hours.
Description
Technical Field
The invention relates to the field of metal pigments for wave-absorbing coatings, in particular to a preparation method of novel high-weather-resistance resin-coated magnetic metal powder.
Background
Carbonyl iron powder is an important magnetic metal powder, has high saturation magnetization and low coercive force, and is often used as a functional metal pigment of radar wave-absorbing coating. However, the flaky carbonyl iron powder is active in property and is very easy to generate oxidation corrosion, and particularly, the flaky carbonyl iron powder can generate serious corrosion problem when used in humid, salt fog and acidic environments, and the electromagnetic property of the flaky carbonyl iron powder is seriously weakened by the formation of corrosion products, so that the application of the flaky carbonyl iron powder is greatly limited. Therefore, it is very urgent to achieve long-term chemical stability and electrical and magnetic stability by surface modification of flaky carbonyl iron powder.
At present, the coating modification of carbonyl iron powder by a surface treatment technology is an effective method for improving the weather resistance of powder, and inorganic silicon dioxide is generally adopted in the industry to carry out surface coating modification on the carbonyl iron powder. Patent CN100409979C uses inorganic nano silica to coat the surface of carbonyl iron powder, which aims to reduce the imaginary part of magnetic permeability and realize low loss. The carbonyl iron powder coated by the method has a large number of tiny particles on the surface, so that the surface of the powder is loose and porous, corrosive media such as water vapor, oxygen, chloride ions, sodium ions and the like cannot be isolated, and the corrosion protection of the carbonyl iron powder is not facilitated. Patent CN103007845B provides Fe @ SiO prepared by sol-gel method aiming at spherical iron powder 2The thickness of a coating layer formed by the method is not uniform in the core-shell structure, and long-time corrosion protection of carbonyl iron powder is difficult to realize. Patent CN112563010AA silicon dioxide coating layer with the thickness of 10-100nm is formed on the surface of the iron powder, although the functional coating test piece prepared by the method can realize no rusty spot on the surface after a salt spray corrosion experiment for 1500 h and 1000 h, the magnetic permeability imaginary part and the dielectric constant imaginary part of the carbonyl iron powder are obviously deteriorated by adopting the surface treatment of the silicon dioxide, so that the performance of the wave-absorbing coating prepared by the iron powder coated by the silicon dioxide can not meet the actual use requirement.
Disclosure of Invention
Aiming at the problems or the defects, the invention provides a preparation method of high-weather-resistance novel resin-coated magnetic metal powder, and the magnetic metal powder prepared by the method can ensure that the electromagnetic parameters are not obviously reduced and has long-time salt spray resistance.
A preparation method of high weather-resistant novel resin-coated magnetic metal powder comprises the following steps:
step 1, dissolving a surfactant in an ester solvent at room temperature to obtain a mixture.
And 2, dispersing magnetic metal powder in the mixture obtained in the step 1, dripping acrylic acid at 40-60 ℃, stirring uniformly, sequentially adding an organic cross-linking agent and an organic peroxide initiator for a cross-linking reaction, wherein the reaction atmosphere is a nitrogen environment.
And 3, after the crosslinking reaction in the step 2 is finished, cooling to room temperature, washing and filtering the crosslinked product by using an ester solvent, and then washing and filtering by using absolute ethyl alcohol.
And 4, carrying out heat treatment on the product (the magnetic metal powder with the surface coated and modified) obtained in the step 3 at the temperature of 60-100 ℃ to obtain the magnetic metal powder with the uniform and densely coated surface, wherein the solid content of the magnetic metal powder is 85-95%.
Further, the magnetic metal powder is sheet carbonyl iron powder.
Further, the surfactant in the step 1 is one or more of glycine, alanine, p-aminobenzoic acid and hexadecyl trimethyl ammonium bromide, and the concentration of the surfactant is 0.05-2.00 g/mL.
Further, the ester solvents in steps 1 and 3 are one or two of methyl acetate, butyl acetate, ethyl propionate and ethyl butyrate.
Further, the acrylic acid in the step 2 is one or more of methyl acrylate, butyl acrylate, ethyl methacrylate and n-butyl methacrylate; according to the mass percentage, the adding amount of the acrylic acid is 0.5-1.0% of the magnetic metal powder.
Further, the organic cross-linking agent in the step 2 is one or more of gamma-aminopropyl triethoxysilane, gamma-methacryloxypropyl trimethoxysilane, perfluorodecyl trimethoxysilane and perfluorooctyl triethoxysilane; the addition amount of the organic cross-linking agent is 0.1-0.3% of the magnetic metal powder by mass percent.
Further, the organic peroxide initiator in the step 2 is one of cumene hydroperoxide, tert-butyl hydroperoxide, dibenzoyl peroxide, lauroyl peroxide and di-tert-butyl peroxide; the addition amount of the organic peroxide initiator is 0.1-0.3% of the magnetic metal powder in percentage by mass.
Further, the crosslinking reaction time in the step 2 is 0.5-2 hours, and the reaction is carried out in a stirring state.
Further, the heat treatment time in the step 4 is 8-24 hours.
The invention coats the magnetic metal powder by selecting the resin which is a material not used for modifying the magnetic metal powder in the industry, and the weather resistance of the coated magnetic metal powder is enhanced by designing the process conditions, and meanwhile, the magnetic conductivity imaginary part and the dielectric constant imaginary part do not cause obvious deterioration. The method has the advantages of simple and mature process, strong operability and lower cost, and is suitable for large-scale production. The coated magnetic metal powder has uniform and compact surface, the electromagnetic parameter change of the coated magnetic metal powder is smaller, the weather resistance is obviously enhanced compared with the similar coated magnetic metal powder (such as carbonyl iron powder), and the salt spray resistance time of the prepared coated magnetic metal powder for manufacturing the wave-absorbing coating can reach more than 3000 hours.
Drawings
FIG. 1 is an SEM image of a coated flaky carbonyl iron powder of example 1;
FIG. 2 is a Tafel plot of the flaky carbonyl iron powder of example 1 before and after coating;
FIG. 3 is an SEM image of coated flaky carbonyl iron powder of example 2;
FIG. 4 is a Tafel plot before and after coating with the flaky carbonyl iron powder of example 2;
FIG. 5 is an SEM photograph of coated flaky carbonyl iron powder in example 3;
FIG. 6 is a Tafel plot before and after coating with the flaky carbonyl iron powder of example 3;
FIG. 7 is an SEM photograph of coated flaky carbonyl iron powder of example 4;
FIG. 8 is a Tafel plot before and after coating with the flaky carbonyl iron powder of example 4;
FIG. 9 is a schematic flow chart of the present invention.
Detailed Description
The technical solutions of the present invention will be described in further detail below with reference to the embodiments and the drawings, but the present invention is not limited thereto.
Example 1:
step 1, dissolving 2g of glycine and 3g of alanine in a mixed solution of 40ml of butyl acetate and 60ml of ethyl propionate at the same time, and fully and uniformly stirring to obtain a mixed solution A.
And 2, dispersing 50g of flaky carbonyl iron powder in the mixed solution A, heating to 40 ℃, slowly adding 0.25g of methyl acrylate, and then sequentially adding 0.05g of organic cross-linking agent gamma-aminopropyltriethoxysilane, wherein the reaction atmosphere is a nitrogen environment, the stirring speed is 250 revolutions per minute, and the stirring time is 0.5 hour.
And 3, after the crosslinking reaction in the step 2 is finished, cooling to room temperature, washing and filtering the crosslinked product by butyl acetate, and then washing and filtering by absolute ethyl alcohol.
And 4, carrying out heat treatment on the flaky carbonyl iron powder obtained in the step 3 at the temperature of 60 ℃ for 8 hours to obtain flaky carbonyl iron powder with uniform and densely-coated surface. FIG. 1 is an SEM image of an example of a coated flaky carbonyl iron powder, and Table 1 shows the SEM image before coatingThe change of the electromagnetic parameters of the powder after modification can be seen to be very small, fig. 2 is a tafel curve of the powder after coating, and table 2 is the corresponding corrosion parameters in the tafel curve. The open-circuit voltage of the powder coated by the case one is increased to 0.063V, the electrode potential is increased to-0.054V, the corrosion current density is increased by two orders of magnitude, and the polarization impedance is increased to 27119 omega/cm2. The neutral salt spray resistant time of the wave-absorbing coating prepared by the case one coated powder reaches more than 3200 hours.
Table 1: example 1 electromagnetic parameter changes before and after powder coating
Table 2: example 1 Corrosion parameter Change before and after powder coating
Open circuit voltage | Potential of electrode | Density of corrosion current | Polarization resistor | |
Raw powder | -0.653V | -0.868V | 1.493×10-4 A/cm2 | 87.1Ω/cm2 |
Example 1 coated powder | 0.063V | -0.054V | 1.981×10-6 A/cm2 | 27119Ω/cm2 |
Example 2:
step 1, simultaneously dissolving 5g of p-aminobenzoic acid and 7.5g of alanine in a mixed solution of 50ml of butyl acetate and 75ml of ethyl butyrate, and fully and uniformly stirring to obtain a mixed solution A.
And 2, dispersing 100g of sheet carbonyl iron powder in the mixed solution A, heating to 50 ℃, slowly adding 0.75g of methyl acrylate, and then sequentially adding 0.1g of organic cross-linking agent perfluorodecyl trimethoxy silane, wherein the reaction atmosphere is a nitrogen environment, the stirring speed is 250 revolutions per minute, and the stirring time is 0.6 hour.
And 3, after the crosslinking reaction in the step 2 is finished, cooling to room temperature, washing and filtering the crosslinked product by butyl acetate, and washing and filtering by absolute ethyl alcohol.
And 4, carrying out heat treatment on the flaky carbonyl iron powder obtained in the step 3 at the temperature of 75 ℃ for 10 hours to obtain flaky carbonyl iron powder with uniform and densely-coated surface. Fig. 3 is an SEM image of the flaky carbonyl iron powder after the second coating, table 3 is the change of the electromagnetic parameters of the powder before and after the coating, fig. 4 is a tafel curve of the powder after the second coating, and table 4 is the corresponding corrosion parameters in the tafel curve. The open-circuit voltage of the powder coated by case two is increased to 0.049V, the electrode potential is increased to-0.045V, the corrosion current density is increased by two orders of magnitude, and the polarization impedance is increased to 36180 omega/cm 2. The neutral salt spray resistant time of the wave-absorbing coating prepared by the case two coating powder reaches more than 3400 hours.
Table 3: example 2 electromagnetic parameter changes before and after powder coating
Table 4: example 2 Corrosion parameters before and after powder coating
Open circuit voltage | Potential of electrode | Density of corrosion current | Polarization resistor | |
Raw powder | -0.653V | -0.868V | 1.493×10-4 A/cm2 | 87.1Ω/cm2 |
Example 2 coated powder | 0.049V | -0.045V | 1.240×10-6 A/cm2 | 36180Ω/cm2 |
Example 3:
step 1, dissolving 8g of hexadecyl trimethyl ammonium bromide in a mixed solution of 30ml of butyl propionate and 50ml of ethyl butyrate, and fully and uniformly stirring to obtain a mixed solution A.
And 2, dispersing 80g of sheet carbonyl iron powder in the mixed solution A, heating to 75 ℃, slowly adding 0.8g of n-butyl methacrylate, and then sequentially adding 0.15g of organic cross-linking agent perfluorodecyl trimethoxy silane, wherein the reaction atmosphere is a nitrogen environment, the stirring speed is 250 revolutions per minute, and the stirring time is 0.5 hour.
And 3, after the crosslinking reaction in the step 2 is finished, cooling to room temperature, washing and filtering the crosslinked product by butyl acetate, and washing and filtering by absolute ethyl alcohol.
And 4, carrying out heat treatment on the flaky carbonyl iron powder obtained in the step 3 at the temperature of 80 ℃ for 17 hours to obtain flaky carbonyl iron powder with uniform and densely coated surface. Fig. 5 is an SEM image of the case of the sheet carbonyl iron powder after three coating, table 5 is the change of the electromagnetic parameters of the powder before and after coating, fig. 6 is the tafel curve of the case of the powder after three coating, and table 6 is the corresponding corrosion parameters in the tafel curve. After the three cases are adopted, the open-circuit voltage of the powder is increased to 0.011V, the electrode potential is increased to-0.103V, the corrosion current density is increased by two orders of magnitude, and the polarization impedance is increased to 35164 omega/cm 2. The neutral salt spray resistant time of the wave-absorbing coating prepared by the case one coated powder reaches more than 3500 hours.
Table 5: example 3 variation of electromagnetic parameters before and after powder coating
Table 6: example 3 Corrosion parameter Change before and after powder coating
Open circuit voltage | Potential of electrode | Density of corrosion current | Polarization resistor | |
Raw powder | -0.653V | -0.868V | 1.493×10-4 A/cm2 | 87.1Ω/cm2 |
Example 3 coated powder | 0.011V | -0.103V | 1.220×10-6 A/cm2 | 35164Ω/cm2 |
Example 4:
step 1, dissolving 4g of hexadecyl trimethyl ammonium bromide and 8g of p-aminobenzoic acid in 250ml of mixed solution of ethyl butyrate, and fully and uniformly stirring to obtain mixed solution A.
And 2, dispersing 200g of sheet carbonyl iron powder in the mixed solution A, heating to 80 ℃, slowly adding 1.8g of n-butyl methacrylate, and then sequentially adding 0.2g of organic cross-linking agent perfluorodecyl trimethoxy silane and 0.6g of gamma-aminopropyl triethoxysilane, wherein the reaction atmosphere is a nitrogen environment, the stirring speed is 300 revolutions per minute, and the stirring time is 2 hours.
And 3, after the crosslinking reaction in the step 2 is finished, cooling to room temperature, washing and filtering the crosslinked product by butyl acetate, and washing and filtering by absolute ethyl alcohol.
Step 4, the flaky carbonyl iron obtained in the step 3The powder is subjected to heat treatment for 24 hours at the temperature of 80 ℃ to obtain the flaky carbonyl iron powder with uniform and dense coating on the surface. Fig. 7 is an SEM image of the case of the four-coated flaky carbonyl iron powder, table 7 is the change of the electromagnetic parameters of the powder before and after coating, fig. 8 is the tafel curve of the case of the four-coated powder, and table 8 is the corresponding corrosion parameters in the tafel curve. After the case four is adopted, the open-circuit voltage of the powder is increased to 0.059V, the electrode potential is increased to-0.040V, the corrosion current density is increased by two orders of magnitude, and the polarization impedance is increased to 19965 omega/cm 2. The wave-absorbing coating prepared by using the four-case coated powder has the neutral salt spray resistance time of more than 3100 hours.
Table 7: example 4 variation of electromagnetic parameters before and after coating of powder
Table 8: example 4 Corrosion parameter Change before and after powder coating
Open circuit voltage | Potential of electrode | Density of corrosion current | Polarization resistor | |
Raw powder | -0.653V | -0.868V | 1.493×10-4 A/cm2 | 87.1Ω/cm2 |
Example 4 coated powder | 0.059V | -0.040V | 2.118×10-6 A/cm2 | 19965Ω/cm2 |
As can be seen by the above examples: the method has the advantages of simple and mature process, strong operability and lower cost, and is suitable for large-scale production. The coated flaky carbonyl iron powder prepared by the embodiment has uniform and compact surface, small change of electromagnetic parameters and obviously enhanced weather resistance, and the salt spray resistance time of the wave-absorbing coating prepared by the embodiment can reach more than 3000 hours. Namely, the modified magnetic metal powder (flaky carbonyl iron powder) has high weather resistance and good magnetic performance, and provides a new excellent scheme for preparing high-performance modified magnetic metal powder (radar wave absorber).
Claims (9)
1. A preparation method of novel high-weather-resistance resin-coated magnetic metal powder is characterized by comprising the following steps:
step 1, dissolving a surfactant in an ester solvent at room temperature to obtain a mixture;
step 2, dispersing magnetic metal powder in the mixture obtained in the step 1, dropwise adding acrylic acid at 40-60 ℃, stirring uniformly, and then sequentially adding an organic cross-linking agent and an organic peroxide initiator for a cross-linking reaction, wherein the reaction atmosphere is a nitrogen environment;
Step 3, after the crosslinking reaction in the step 2 is finished, cooling to room temperature, washing and filtering the crosslinked product by using an ester solvent, and then washing and filtering by using absolute ethyl alcohol;
and 4, carrying out heat treatment on the product obtained in the step 3 at the temperature of 60-100 ℃ to obtain magnetic metal powder with a uniform and densely coated surface, wherein the solid content of the magnetic metal powder is 85-95%.
2. The method for preparing the highly weather-resistant novel resin-coated magnetic metal powder as claimed in claim 1, wherein: the magnetic metal powder is sheet carbonyl iron powder.
3. The method for preparing the highly weather-resistant novel resin-coated magnetic metal powder as claimed in claim 1, wherein: the surfactant in the step 1 is one or more of glycine, alanine, p-aminobenzoic acid and hexadecyl trimethyl ammonium bromide, and the concentration of the surfactant is 0.05-2.00 g/mL.
4. The method for preparing the highly weather-resistant novel resin-coated magnetic metal powder as claimed in claim 1, wherein: the ester solvents in the steps 1 and 3 are one or two of methyl acetate, butyl acetate, ethyl propionate and ethyl butyrate.
5. The method for preparing the highly weather-resistant novel resin-coated magnetic metal powder as claimed in claim 1, wherein: the acrylic acid in the step 2 is one or more of methyl acrylate, butyl acrylate, ethyl methacrylate and n-butyl methacrylate; according to the mass percentage, the adding amount of the acrylic acid is 0.5-1.0% of the magnetic metal powder.
6. The method for preparing the highly weather-resistant novel resin-coated magnetic metal powder as claimed in claim 1, wherein: the organic cross-linking agent in the step 2 is one or more of gamma-aminopropyl triethoxysilane, gamma-methacryloxypropyl trimethoxysilane, perfluorodecyl trimethoxysilane and perfluorooctyl triethoxysilane; the addition amount of the organic cross-linking agent is 0.1-0.3% of the magnetic metal powder by mass percent.
7. The method for preparing the highly weather-resistant novel resin-coated magnetic metal powder as claimed in claim 1, wherein: the organic peroxy initiator in the step 2 is one of cumene hydroperoxide, tert-butyl hydroperoxide, dibenzoyl peroxide, lauroyl peroxide and di-tert-butyl peroxide; the addition amount of the organic peroxide initiator is 0.1-0.3% of the magnetic metal powder in percentage by mass.
8. The method for preparing the highly weather-resistant novel resin-coated magnetic metal powder as claimed in claim 1, wherein: the crosslinking reaction time in the step 2 is 0.5-2 hours, and the reaction is carried out in a stirring state.
9. The method for preparing the highly weather-resistant novel resin-coated magnetic metal powder as claimed in claim 1, wherein: and the heat treatment time in the step 4 is 8-24 hours.
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CN117773102A (en) * | 2024-02-28 | 2024-03-29 | 西北工业大学 | Silicon aryne resin coated magnetic metal absorbent and preparation method and application thereof |
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CN117773102B (en) * | 2024-02-28 | 2024-05-24 | 西北工业大学 | Silicon aryne resin coated magnetic metal absorbent and preparation method and application thereof |
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